Jenq Gong Duh

Low temperature sintering and crystallisation behaviour of low loss anorthite-based glass-ceramics

Anorthite-based glass-ceramics including TiO2 as nucleating agent were melted and quenched in this study. The effect of particle size on the sintering behaviour of glass powders was investigated in order to obtain low-temperature sintered glass-ceramics. Anorthite glass-ceramic starts to densify at the transition temperature of glass (Tg = 770°C) and is fully sintered before the crystallisation occurrence (880°C). Therefore, a dense and low-loss glass-ceramic with predominant crystal phase of anorthite is achieved by using fine glass powders (D50 = 0.45 μm) fired at 900°C. The as-sintered density approaches 99% theoretical density and the apparent porosity is as low as 0.05 Vol%. The dense and crystallized anorthite-based glass-ceramic exhibits a fairly low dielectric loss of 4 × 10−4 at 1 MHz and a thermal expansion coefficient of 4.5 × 10−6°C−1. Furthermore, the microwave characteristics were measured at 10 GHz with the results of K = 9.8, Qf = 2250, and temperature coefficient of resonant frequency τf = −30 ppm/°C.

Effect of nitride film coatings on cell compatibility.

OBJECTIVEnTo evaluate the cytotoxicity of nickel-based alloy surfaces after nitride film coatings.nnnMETHODSnA total of 120 disc-shaped specimens (1.5 x 12.0mm) were prepared from nickel (Ni) alloy ingots and metallurgically ground with silicon carbide (SiC) sandpaper to 1200 grit and used as the ground group. Ninety specimens from the ground group were selected and further polished with 1.0 microm aluminum powder slurry and assigned as the polished group. Titanium nitride (TiN) and titanium-aluminum nitride (TiAlN) film coatings were deposited onto 30 polished specimens each by a reactive radio frequency magnetron sputter deposition system and used as coated groups, respectively. The morphological changes and cytoskeleton of tested human gingival fibroblasts were observed using fluorescence microscopy at 3h and 24h time periods, respectively. An MTT assay was used to assess cell viability at 24h. The results were statistically analyzed (n=5, ANOVA, Scheffe, p<0.05).nnnRESULTSnAfter 3h of incubation, cells began to spread on the test surfaces. Spindle-shaped fibroblasts with well-developed cytoskeleton and distinct actin fibers were observed at the 24h incubation point on the polished and coated specimens. Results of the MTT assay revealed that the TiN and TiAlN film coated groups were significantly higher in cell proliferation and viability than the polished and control groups (p<0.05).nnnSIGNIFICANCEnThe biocompatibility of Ni-based alloy was increased significantly after nitride film coating.

Corrosion of aluminium nitride substrates in acid, alkaline solutions and water

Aluminium nitride substrates were immersed in acid, basic solutions and deionized water for 1–120 h at room temperature. The corrosion rates are higher in basic solutions (NaOH and KOH) than those in acid solutions (CH3COOH, HCOOH, HNO3, HCl and H2SO4) and deionized water. The weight loss of AIN corroded in alkali aqueous reaches 70% and results in an increase in surface roughness ranging from 10 nm to 7 μm after 3 days corrosion. However, the weight loss in acid solution is only 1/700 of the alkali case. Violent chemical reactions between AIN and basic solutions were observed. Na2O, or Na2Al2O4·6H2O, is the intermediate product, and NaOH is a catalytic agent of the reaction. The surface morphology of the AIN etched by alkaline solutions is coral-like in microscopic view and appears like hills. In contrast, only several atomic layers of AIN surface are etched off in acid solutions and in deionized water. The lightly etched surface is mirror-like and flat, and the shapes of the grains are visible under the microscope, as the corrosion rate of each AIN grain varies with different crystal orientations. Consequently, after etching in acid solutions, the resulting microscopic surface morphology looks like a map of a jigsaw puzzle.

Morphology and electrochemical behavior of Ag–Cu nanoparticle-doped amalgams

The aim of this study was to introduce Ag-Cu phase nanopowder as an additive to improve the corrosion behavior of dental amalgams. A novel Ag-Cu nanopowder was synthesized by the precipitation method. An amalgam alloy powder (World-Cap) was added and mixed with 5 wt.% and 10 wt.% of Ag-Cu nanopowders, respectively, to form experimental amalgam alloy powders. The original alloy powder was used as a control. Alloy powders were examined using X-ray diffraction, transmission electron microscopy (TEM), scanning electron microscopy and electron probe microanalysis. Amalgam disk specimens of metallurgically prepared were tested in 0.9% NaCl solution using electrochemical methods. The changes in the corrosion potential and anodic polarization characteristics were determined. Corrosion potential data were analyzed statistically (n=3, analysis of variance, Tukeys test, p<0.05). The diameters of lamellar structure Ag-Cu nanoparticles were measured to be approximately 30 nm. The composition of the Ag-Cu nanoparticles determined by TEM-energy-dispersive spectroscopy was 56.28 at.% Ag-43.72 at.% Cu. A light-shaded phase was found mixing with dark Cu-Sn reaction particles in the reaction zones of Ag-Cu nanoparticle-doped amalgams. The Ag-Cu nanoparticle-doped amalgams exhibited zero current potentials more positive than the control (p<0.05) and no current peak was observed at -325mV that related to Ag-Hg phase and Cu6Sn5 phase in anodic polarization curves. The results indicated that the corrosion resistance of high-copper single-composition amalgam could be improved by Ag-Cu nanoparticle-doping.

The effect of sintering conditions on the grain growth of the BaTiO3-based GBBL capacitors

BaTiO3-based grain-boundary barrier layer capacitors are prepared by a conventional ceramic fabrication process with SiO2, Dy2O3 and Nb2O5 dopants. A two-stage sintering process is employed to investigate the influence of the sintering conditions on the grain size of the BaTiO3 ceramics. The reducing sintering atmosphere or reducing catalytic dopant decreases the apparent eutectic temperature of the BaTiO3 ceramics. The decrease in the eutectic temperature associated with abnormal grain growth is related to the oxygen partial pressure during sintering. By properly employing the sintering temperature profile and the sintering atmosphere, a desirable microstructure with controlled grain growth could be achieved.

Microstructural Evaluation of High Oxidation Resistant CrAlSiN Hard Coating at Elevated Temperature in Air Atmosphere

CrAlSiN hard coatings were fabricated on the Si substrate from metallurgical Cr0.45Al0.45Si0.10 alloy target by reactive r.f. magnetron sputtering. The oxidation resistance of CrAlSiN coatings was investigated after annealing at temperatures between 900 and 1100°C for 1 hr in air. The phase identification and microstructure of CrAlSiN coatings after heat treatment were analyzed by X-ray diffraction (XRD). The hardness of CrAlSiN coating after heat treatment at 900oC for 1hr in air is slightly decreased from 30.2GPa to 28.3±1.3GPa, which was caused by the thin oxide formation on the surface of the film. The microstructure of CrAlSiN coating after heat treatment at 1000oC from 1 hr analyzed by TEM revealed two types of layer feature, including the nanocrystalline grain embedded in the Al-riched amorphous layer and reaction interface with relative high content of Si.

The Effect of Tungsten Addition on the Thermal Stability and Microstructure in the Electroless Ni-P-W Composite Coating

Ni-P-W composite deposit on the mild steel substrate was derived by the electroless process. The composition of the eletroless coating was Ni-10.7wt.%P-8.7wt%W analyzed by electron probe microanalysis (EPMA). The coating was annealed at various temperatures from 350oC to 600oC for 4h and the structure at different heat-treated temperature was studied by X-ray diffraction, and transmission electron microscope (TEM). The crystallization behavior was evaluated by the differential scanning calorimeter analysis with continuously heating from room temperature to 550oC at different heating rates. The hardness at all depths of the coating on the substrate could be acquired by the nanoindentation. From the DSC analysis, the onset temperature and crystallization temperature were 397.7oC and 405.5oC, respectively, at the heating rate of 10oC/min. The activation energy of the Ni-P-W coating was 307 kJ/mol analyzed by Kissinger, and Augis and Bennett methods with different heating rates. The Ni-P-W coating showed an amorphous structure in the as-deposited state and exhibited a relatively low hardness of approximately 6.8 GPa. As temperature was raised to 380oC, the hardness was slightly increased to 8.7 GPa due to the partial precipitation of Ni and Ni3P in the amorphous matrix. On heating to 500oC for 4 h, the hardness reached the maximum value of 12.3 GPa with a grain size of 33.1 nm and followed by gradual degradation above 500oC.

Surface treatment of the lithium boron oxide coated LiMn2O4 cathode material in Li-ion battery

Surface modification on the electrode has a vital impact on lithium-ion batteries, and it is essential to probe the mechanism of the modified film on the surface of the electrode. In this study, a Li2O-2B2O3 film was coated on the surface of the cathode material by solution method. The cathode powders derived from co-precipitation method were calcined with various weight percent of the surface modified glass to form fine powder of single spinel phase with different particle size, size distribution and morphology. The thermogravimetry/differential thermal analysis was used to evaluate the appropriate heat treatment temperature. The structure was confirmed by the X-ray diffractometer along with the composition measured by the electron probe microanalyzer. From the field emission scanning electron microscope image and Laser Scattering measurements, the average particle size was in the range of 7-8µm. The electrochemical behavior of the cathode powder was examined by using two-electrode test cells consisted of a cathode, metallic lithium anode, and an electrolyte of 1M LiPF6. Cyclic charge/discharge testing of the coin cells, fabricated by both coated and un-coated cathode material, provided high discharge capacity. Furthermore, the coated cathode powder showed better cyclability than the un-coated one after the cyclic test. The introduction of the glass-coated cathode material revealed high discharge capacity and appreciably decreased the decay rate after cyclic test.

Effect of the Thickness of Cr Interlayer on the High-Frequency Characteristics of FeCoTa/Cr/FeCoTa Multilayers

The effect of non-ferromagnetic Cr interlayer on the high-frequency ferromagnetic properties (HFFMPs) was investigated by use of FeCoTa/Cr/ FeCoTa triple layered films. In conventional thought, the metal interlayer gives rise to a high eddy current loss and therefore a deteriorated HFFMP. However, it is found that HFFMPs depend on the thickness of Cr interlayer. The HFFPMs are improved by Cr-interlayer with a thickness less than 12 nm (sample C1). Comparing with the Cr-interlayer-free FeCoHf single layered film (sample C0), the magnetic anisotropy field of C1 dramatically increases from 185 Oe for C0 to 558 Oe for C1. As a consequence, a high ferromagnetic resonance frequency over than 3 GHz is achieved for sample C1. When the thickness of Cr-interlayer is more than 120 nm (C2), the HFFMPs are reduced due to the increase of eddy current loss and magnetic decoupling between the ferromagnetic layers.

Synthesis and Characterization of LiNixCoyMn1-x-yO2 as a Cathode Material for Lithium Ion Batteries

The newly developed LiNi0.6Co0.4-xMnxO2 (0.1 < x < 0.3) cathode materials were synthesized by calcining the mixture of NixCoyMn1-x-y(OH)2 and Li2CO3 at 900-940 oC for 15 hr in flowing O2 atmosphere. The NixCoyMn1-x-y(OH)2 precursor was obtained by the chemical co-precipitation method at the pH value controlled by the concentration of NaOH, NH4OH and transition metal sulfate solution. The X-ray diffraction patterns indicated the pure layered hexagonal structure LiNi0.6Co0.4-xMnxO2. The electrochemical behavior of LiNixCoyMn1-x-yO2 powder was examined by using test cells cycled within the voltage range 3-4.3 V at the 0.1C rate for the first cycle and then at the 0.2C rate afterwards. LiNixCoyMn1-x-yO2 cathode materials showed good initial discharge capacity (165-180 mAh/g) and cycling performance. The fading rate was less than 5 % after 20 cycling test. It is demonstrated that LiNixCoyMn1-x-yO2 electrode should exhibit great potential for the future application in lithium-ion battery cathode material.